5-cyano-2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid → 2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-5-carbonitrile

HRID 2401174노트

반응식

HRID 2401174 반응식
[C:1]([C:3]1[CH:4]=[C:5]2[C:11](C(O)=O)=[C:10]([C:15]([F:18])([F:17])[F:16])[NH:9][C:6]2=[N:7][CH:8]=1)#[N:2]>O.CN1CCCC1=O>[F:18][C:15]([F:16])([F:17])[C:10]1[NH:9][C:6]2=[N:7][CH:8]=[C:3]([C:1]#[N:2])[CH:4]=[C:5]2[CH:11]=1

참가 물질

4

반응물 1

HCID 671123375-cyano-2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid2회

생성물 1

HCID 671115072-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-5-carbonitrile수율 61.1%

시약·촉매·용매 2

HCID 962Water용매2회HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
120 °C

실험 절차

5-Cyano-2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid (Intermediate 3, 2.49 g, 9.76 mmol) was dissolved in water (36 mL) and N-methyl-2-pyrrolidone (48 mL). The resulting mixture was heated at 120° C. for 18 hours. The reaction mixture was allowed to cool to room temperature and diluted with water. The resulting precipitate was collected by filtration, washed with water and dried under high vacuum at 40° C. for 5 hours to give the title compound as a white solid (1.26 g);

후처리

  1. temperatureto cool to room temperature
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customdried under high vacuum at 40° C. for 5 hours

출처 및 근거

ORD 기록
ord-2f28891b36df4361b27dfb5b76c5c03b
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796283B2

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